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    ICP-OES法同时测定煤中11种微量元素

    Simultaneous determination of 11 trace elements in coal by inductively coupled plasma-optical emission spectrometry

    • 摘要: 为实现煤中多种微量元素的批量快速测定,煤样经高温灰化、盐酸-氢氟酸-高氯酸三元体系溶解、盐酸提取后,使用电感耦合等离子体发射光谱(ICP-OES)同时测定煤中镓钍钒磷铜钴镍锌铅铬镉11种微量元素。在对样品分解方法、射频功率、分析谱线和积分点数合理选择的基础上,通过离峰扣背景法消除了各种光谱干扰对测定的影响,建立了采用ICP-OES同时测定煤中镓钍钒磷铜钴镍锌铅铬镉11种微量元素的实验方法。方法检出限为0.03~1.17μg/g,方法精密度(n=11)0.32%~3.19%,土壤国家标准物质的分析测定值与标准值吻合较好。与传统化学方法相比,该方法快速准确,提高了分析效率,满足煤质分析的一般要求。

       

      Abstract: To quickly determine microelements of coal in batch,the coal sample was ashed first at high temperature,then the product was dissolved by the mixture of HCl,HF and HCl O4,the third step was to extract the microelements with HCl. The microelements which were Ga,Th,V,P,Cu,Co,Ni,Zn,Pb,Cr,Cd were determined with ICP- OES( Inductively Coupled Plasma- Optical Emission Spectrometry).With reasonable sample dissolution methods,radio- frequency power,analytical spectral line and experimental data,the influence of spectral interference on determination was eliminated by off- peak background deduction method,meanwhile,the 11 kinds of microelements could be determined by ICP- OES at the same time. The detection limits for the elements was 0. 03 ~ 1. 17 μg / g. The method was applied to the determination of 11 microelements in Soil National Standard Reference Materials and the results were in agreement with certified values with precision of 0. 32% ~ 3. 19% RSD( n = 11).

       

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